CN106810847A - A kind of antibacterial type polyurethane waterproof material and preparation method thereof - Google Patents
A kind of antibacterial type polyurethane waterproof material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of antibacterial type polyurethane waterproof material, it is made up of the raw material of following weight parts：Toluene di-isocyanate(TDI) 100 120, polyester diol 110 130, dibutyl tin laurate 0.4 1, ethylene bis stearamide 12, palm wax 34, stearic acid 23, sorbitan monooleate 0.5 1, polybenzimidazoles 12, CNT 10 12, octylisothiazolinone 12, Sodium Benzoate 0.4 2, castor oil acid 0.1 0.16, mannitol 68, cumyl peroxide 0.01 0.02, 8 copper quinolinates 23, dihydromethyl propionic acid 24, methyl-silicone oil 0.1 0.3, the present invention uses castor oil acid, polyurethane material after stearic acid modified antibacterial treatment, effectively raise the water resistance of finished product, improve the bin stability of finished product.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of antibacterial type polyurethane waterproof material and preparation method thereof.
Background technology
Polyurethane material is the current best insulation material of performance in the world.Main chain is containing-NHCOO-constitutional repeating unit
One birds of the same feather flock together compound.English abbreviation PU.It is polymerized with hydroxy compounds by isocyanates (monomer).Due to containing highly polar ammonia
Carbamate base, insoluble in non-polar group, with good oil resistivity, toughness, wearability, resistance to ag(e)ing and cohesive.With
Different material can be obtained the material for adapting to wide temperature range, including elastomer, thermoplastic resin and thermosetting resin.Under high temperature
Not hydrolysis, also not alkali-proof medium.
Conventional monomer such as toluene di-isocyanate(TDI), '-diphenylmethane diisocyanate etc..3 classes of polyalcohol point：It is simple polynary
Alcohol (ethylene glycol, glycerine etc.)；Polyester oligomer containing terminal hydroxyl, for preparing PAUR；Containing terminal hydroxyl
Polyether oligomers, for preparing EU.Polymerization is different with material character.First prepared during synthetic elastomer low
Molecular weight dihydroxylic alcohols, then reacted with excess aromatic or aliphatic isocyanates, generation isocyano (- NCO) is end group
Prepolymer, then with polyalcohol chain extension, obtain thermoplastic elastomer；If being crosslinked with diamine chain extension and further, casting type bullet is obtained
Gonosome.Prepolymer hydrazine or diamine chain extension, obtain elastomer；The excessively more performed polymer of isocyanates and catalyst, hair
Infusion mixes, and can directly obtain rigid foam.Such as monomer, polyethers, water, catalyst are mixed, single step reaction can be obtained
To flex foam.Monomer reacts in the solution with polyalcohol, can obtain coating；Adhesive then with polyisocynate monomer and
Low molecular weight polyester or polyethers mix and are reacted when in use.
Polyurethane elastomer is used as roller, conveyer belt, flexible pipe, auto parts, sole, synthetic leather, electric wire and doctor
Manually internal organs etc.；Flexible foam be used for vehicle, room, the pad of clothes, hard foam be used as heat-insulated, sound-absorbing, packaging,
Insulation and low ratio foamed synthetic wood, coating are used for advanced vehicle, furniture, wood and metal protection, pond dam and building antiseepage
Leakage material, and fabric coating etc..Adhesive has good adhesion strength to metal, glass, ceramics, leather, fiber etc..In addition
Polyurethane may also be fabricated which emulsion, magnetic material etc.；But conventional urethane store materials stability is bad, antibacterial anti-corrosive properties are poor,
Cause service life low.
The content of the invention
Defect and deficiency it is an object of the invention to be directed to prior art, there is provided a kind of antibacterial type polyurethane waterproof material
And preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of antibacterial type polyurethane waterproof material, it is made up of the raw material of following weight parts：
Toluene di-isocyanate(TDI) 100-120, polyester diol 110-130, dibutyl tin laurate 0.4-1, ethylene are double
Stearmide 1-2, palm wax 3-4, stearic acid 2-3, sorbitan monooleate 0.5-1, polybenzimidazoles 1-2, CNT 10-
12nd, octylisothiazolinone 1-2, Sodium Benzoate 0.4-2, castor oil acid 0.1-0.16, mannitol 6-8, cumyl peroxide
0.01-0.02, copper 8-quinolinolate 2-3, dihydromethyl propionic acid 2-4, methyl-silicone oil 0.1-0.3.
A kind of preparation method of antibacterial type polyurethane waterproof material, comprises the following steps：
(1) by above-mentioned mannitol insulated and stirred 10-20 minutes at 76-80 DEG C, above-mentioned octylisothiazolinone is added, after
Continuous insulated and stirred 4-10 minutes, adds above-mentioned methyl-silicone oil, is passed through nitrogen, insulated and stirred 40-50 minutes at 180-200 DEG C,
Above-mentioned Sodium Benzoate is added, is stirred to normal temperature, obtain antibacterial alcohol liquid；
(2) above-mentioned polybenzimidazoles is added in the absolute ethyl alcohol of 10-15 times of its weight, is stirred, rise high-temperature
It is 70-75 DEG C, adds above-mentioned sorbitan monooleate, insulated and stirred 4-9 minutes, obtains alcohol dispersion liquid；
(3) above-mentioned CNT is taken, is added in the salpeter solution that concentration is 96-98%, it is ultrasonic 20-30 minutes, add
Above-mentioned copper 8-quinolinolate, it is 60-65 DEG C to rise high-temperature, and insulated and stirred 10-20 minutes, precipitation was washed in filtering 2-3 times,
It is vacuum dried 1-2 hours at 80-90 DEG C, obtains antibacterial CNT；
(4) above-mentioned stearic acid, castor oil acid are mixed, is added in the deionized water of 67-80 times of compound weight, stirred
Uniformly, above-mentioned ethylene bis stearamide is added, is stirred, obtain acid amides dispersion liquid；
(5) above-mentioned antibacterial CNT is added in acid amides dispersion liquid, it is ultrasonic 3-4 minutes, obtain CNT acid amides point
Dispersion liquid；
(6) above-mentioned polyester diol is dried 10-11 hours in 100-105 DEG C of vacuum drying chamber, discharging cooling is sent
Enter in reactor, be passed through nitrogen, regulation temperature of reaction kettle is 40-50 DEG C, and toluene di-isocyanate(TDI) is added dropwise, and is incubated after completion of dropping
20-30 minutes, above-mentioned dibutyl tin laurate is added, it is 60-70 DEG C to rise high-temperature, insulation reaction 100-120 minutes, is added
Above-mentioned dihydromethyl propionic acid, insulated and stirred 100-110 minutes, adds above-mentioned antibacterial alcohol liquid, insulated and stirred 50-60 minutes, cooling
To normal temperature, antibacterial polyurethane material is obtained；
(7) above-mentioned cumyl peroxide is added in alcohol dispersion liquid, is stirred, alcohol dispersion liquid must be premixed；
(8) above-mentioned antibacterial polyurethane material is added in CNT acid amides dispersion liquid, is stirred, be passed through nitrogen,
Above-mentioned premix alcohol dispersion liquid is added dropwise, it is 50-60 DEG C to rise high-temperature, insulated and stirred 1-2 hours, is cooled to normal temperature, suction filtration, by filter cake
Washed 2-3 times successively with absolute ethyl alcohol, deionized water, air drying, mixed with remaining each raw material, stirred, feeding extrusion
In machine, melting extrusion, cooling obtains final product the antibacterial type polyurethane waterproof material.
Beneficial effect：Copper 8-quinolinolate, octylisothiazolinone, Sodium Benzoate that the present invention is added etc. can be effective
Finished product polyurethane material bacteriostasis property is improved, CNT is added in acid amides dispersion liquid, can effectively improve carbon nanometer
Dispersiveness of the pipe in polyurethane, reduces and reunites, and improves the stability_intensity of finished-product material, and the present invention is using castor oil acid, hard
Resin acid is modified the polyurethane material after antibacterial treatment, effectively raises the water resistance of finished product, improves the storage stabilization of finished product
Property.
Specific embodiment
Embodiment 1
A kind of antibacterial type polyurethane waterproof material, it is made up of the raw material of following weight parts：
Toluene di-isocyanate(TDI) 100, polyester diol 120, dibutyl tin laurate 0.7, ethylene bis stearamide 1,
Palm wax 3, stearic acid 2, sorbitan monooleate 0.5, polybenzimidazoles 1, CNT 11, octylisothiazolinone 1, benzene first
Sour sodium 0.9, castor oil acid 0.1, mannitol 8, cumyl peroxide 0.02, copper 8-quinolinolate 2, dihydromethyl propionic acid 3, first
Base silicone oil 0.2.
A kind of preparation method of antibacterial type polyurethane waterproof material, comprises the following steps：
(1) by above-mentioned mannitol at 76-80 DEG C insulated and stirred 10 minutes, add above-mentioned octylisothiazolinone, continue
Insulated and stirred 8 minutes, adds above-mentioned methyl-silicone oil, is passed through nitrogen, and insulated and stirred 40 minutes at 200 DEG C add above-mentioned benzene first
Sour sodium, stirs to normal temperature, obtains antibacterial alcohol liquid；
(2) above-mentioned polybenzimidazoles is added in the absolute ethyl alcohol of 10 times of its weight, is stirred, rising high-temperature is
70-75 DEG C, above-mentioned sorbitan monooleate is added, insulated and stirred 8 minutes obtains alcohol dispersion liquid；
(3) above-mentioned CNT is taken, is added in the salpeter solution that concentration is 98%, ultrasound 28 minutes adds above-mentioned 8-
Copper quinolinate, it is 65 DEG C to rise high-temperature, insulated and stirred 17 minutes, and filtering, by precipitation washing 2 times, 1 is vacuum dried at 90 DEG C
Hour, obtain antibacterial CNT；
(4) above-mentioned stearic acid, castor oil acid are mixed, is added in the deionized water of 67-80 times of compound weight, stirred
Uniformly, above-mentioned ethylene bis stearamide is added, is stirred, obtain acid amides dispersion liquid；
(5) above-mentioned antibacterial CNT is added in acid amides dispersion liquid, it is ultrasonic 3-4 minutes, obtain CNT acid amides point
Dispersion liquid；
(6) above-mentioned polyester diol is dried 10 hours in 100-105 DEG C of vacuum drying chamber, discharging cooling, feeding
In reactor, nitrogen is passed through, regulation temperature of reaction kettle is 40 DEG C, and toluene di-isocyanate(TDI) is added dropwise, and 20 points are incubated after completion of dropping
Clock, adds above-mentioned dibutyl tin laurate, and it is 68 DEG C to rise high-temperature, and insulation reaction 100 minutes adds above-mentioned dihydroxymethyl third
Acid, insulated and stirred 100 minutes adds above-mentioned antibacterial alcohol liquid, and insulated and stirred 60 minutes is cooled to normal temperature, obtains antibacterial polyurethane material
Material；
(7) above-mentioned cumyl peroxide is added in alcohol dispersion liquid, is stirred, alcohol dispersion liquid must be premixed；
(8) above-mentioned antibacterial polyurethane material is added in CNT acid amides dispersion liquid, is stirred, be passed through nitrogen,
Above-mentioned premix alcohol dispersion liquid is added dropwise, it is 60 DEG C to rise high-temperature, and insulated and stirred 2 hours is cooled to normal temperature, suction filtration, by filter cake nothing
Water-ethanol, deionized water are washed 3 times successively, air drying, are mixed with remaining each raw material, are stirred, and in feeding extruder, are melted
Melt extrusion, cool down, obtain final product the antibacterial type polyurethane waterproof material.
Embodiment 2
A kind of antibacterial type polyurethane waterproof material, it is made up of the raw material of following weight parts：
Toluene di-isocyanate(TDI) 120, polyester diol 130, dibutyl tin laurate 0.9, ethylene bis stearamide 1,
Palm wax 3, stearic acid 2, sorbitan monooleate 0.8, polybenzimidazoles 1, CNT 10, octylisothiazolinone 1, benzene first
Sour sodium 0.4, castor oil acid 0.1, mannitol 6, cumyl peroxide 0.01, copper 8-quinolinolate 2, dihydromethyl propionic acid 2, first
Base silicone oil 0.1.
A kind of preparation method of antibacterial type polyurethane waterproof material, comprises the following steps：
(1) insulated and stirred 20 minutes, the above-mentioned octylisothiazolinone of addition, continuation insulation at 80 DEG C by above-mentioned mannitol
Stirring 8 minutes, adds above-mentioned methyl-silicone oil, is passed through nitrogen, and insulated and stirred 40 minutes at 200 DEG C add above-mentioned Sodium Benzoate,
Stirring obtains antibacterial alcohol liquid to normal temperature；
(2) above-mentioned polybenzimidazoles is added in the absolute ethyl alcohol of 15 times of its weight, is stirred, it is 75 to rise high-temperature
DEG C, above-mentioned sorbitan monooleate is added, insulated and stirred 9 minutes obtains alcohol dispersion liquid；
(3) above-mentioned CNT is taken, is added in the salpeter solution that concentration is 98%, ultrasound 30 minutes adds above-mentioned 8-
Copper quinolinate, it is 65 DEG C to rise high-temperature, insulated and stirred 20 minutes, and filtering, by precipitation washing 2 times, 1 is vacuum dried at 90 DEG C
Hour, obtain antibacterial CNT；
(4) above-mentioned stearic acid, castor oil acid are mixed, is added in the deionized water of 80 times of compound weight, stirring is equal
It is even, above-mentioned ethylene bis stearamide is added, stir, obtain acid amides dispersion liquid；
(5) above-mentioned antibacterial CNT is added in acid amides dispersion liquid, ultrasound 4 minutes, obtains the dispersion of CNT acid amides
Liquid；
(6) above-mentioned polyester diol is dried 11 hours in 105 DEG C of vacuum drying chamber, discharging cooling, feeding reaction
In kettle, nitrogen is passed through, regulation temperature of reaction kettle is 50 DEG C, and toluene di-isocyanate(TDI) is added dropwise, and 20 minutes are incubated after completion of dropping, plus
Enter above-mentioned dibutyl tin laurate, it is 70 DEG C to rise high-temperature, and insulation reaction 100 minutes adds above-mentioned dihydromethyl propionic acid, protects
Temperature stirring 110 minutes, adds above-mentioned antibacterial alcohol liquid, and insulated and stirred 60 minutes is cooled to normal temperature, obtains antibacterial polyurethane material；
(7) above-mentioned cumyl peroxide is added in alcohol dispersion liquid, is stirred, alcohol dispersion liquid must be premixed；
(8) above-mentioned antibacterial polyurethane material is added in CNT acid amides dispersion liquid, is stirred, be passed through nitrogen,
Above-mentioned premix alcohol dispersion liquid is added dropwise, it is 60 DEG C to rise high-temperature, and insulated and stirred 2 hours is cooled to normal temperature, suction filtration, by filter cake nothing
Water-ethanol, deionized water are washed 3 times successively, air drying, are mixed with remaining each raw material, are stirred, and in feeding extruder, are melted
Melt extrusion, cool down, obtain final product the antibacterial type polyurethane waterproof material.
The above, is only presently preferred embodiments of the present invention, not makes any limit to technical scope of the invention
System, therefore every any trickle amendment, equivalent variations and modification made to above example according to technical spirit of the invention,
Still fall within the range of technical scheme.
Claims (2)
1. a kind of antibacterial type polyurethane waterproof material, it is characterised in that it is made up of the raw material of following weight parts：Toluene two
Isocyanates 100-120, polyester diol 110-130, dibutyl tin laurate 0.4-1, ethylene bis stearamide 1-2, palm fibre
Palmitic acid wax 3-4, stearic acid 2-3, sorbitan monooleate 0.5-1, polybenzimidazoles 1-2, CNT 10-12, octyl group isothiazole
Quinoline ketone 1-2, Sodium Benzoate 0.4-2, castor oil acid 0.1-0.16, mannitol 6-8, cumyl peroxide 0.01-0.02,8- hydroxyl
Base copper 8-hydroxyquinolinate 2-3, dihydromethyl propionic acid 2-4, methyl-silicone oil 0.1-0.3.
2. a kind of preparation method of antibacterial type polyurethane waterproof material as claimed in claim 1, it is characterised in that including following
Step：
(1) by above-mentioned mannitol insulated and stirred 10-20 minutes at 76-80 DEG C, above-mentioned octylisothiazolinone is added, continues to protect
Temperature stirring 4-10 minutes, adds above-mentioned methyl-silicone oil, is passed through nitrogen, insulated and stirred 40-50 minutes at 180-200 DEG C, adds
Above-mentioned Sodium Benzoate, stirs to normal temperature, obtains antibacterial alcohol liquid；
(2) above-mentioned polybenzimidazoles is added in the absolute ethyl alcohol of 10-15 times of its weight, is stirred, liter high-temperature is 70-
75 DEG C, above-mentioned sorbitan monooleate is added, insulated and stirred 4-9 minutes, obtain alcohol dispersion liquid；
(3) above-mentioned CNT is taken, is added in the salpeter solution that concentration is 96-98%, it is ultrasonic 20-30 minutes, add above-mentioned
Copper 8-quinolinolate, it is 60-65 DEG C to rise high-temperature, insulated and stirred 10-20 minutes, filtering, by precipitation washing 2-3 times, in 80-90
It is vacuum dried 1-2 hours at DEG C, obtains antibacterial CNT；
(4) above-mentioned stearic acid, castor oil acid are mixed, is added in the deionized water of 67-80 times of compound weight, stirring is equal
It is even, above-mentioned ethylene bis stearamide is added, stir, obtain acid amides dispersion liquid；
(5) above-mentioned antibacterial CNT is added in acid amides dispersion liquid, it is ultrasonic 3-4 minutes, obtain CNT acid amides dispersion liquid；
(6) above-mentioned polyester diol is dried 10-11 hours in 100-105 DEG C of vacuum drying chamber, discharging cooling, feeding is anti-
Answer in kettle, be passed through nitrogen, regulation temperature of reaction kettle is 40-50 DEG C, and toluene di-isocyanate(TDI) is added dropwise, and 20- is incubated after completion of dropping
30 minutes, above-mentioned dibutyl tin laurate is added, high-temperature is risen for 60-70 DEG C, insulation reaction 100-120 minutes, in addition
Dihydromethyl propionic acid is stated, insulated and stirred 100-110 minutes, above-mentioned antibacterial alcohol liquid is added, insulated and stirred 50-60 minutes, is cooled to
Normal temperature, obtains antibacterial polyurethane material；
(7) above-mentioned cumyl peroxide is added in alcohol dispersion liquid, is stirred, alcohol dispersion liquid must be premixed；
(8) above-mentioned antibacterial polyurethane material is added in CNT acid amides dispersion liquid, is stirred, be passed through nitrogen, be added dropwise
Above-mentioned premix alcohol dispersion liquid, it is 50-60 DEG C to rise high-temperature, insulated and stirred 1-2 hours, is cooled to normal temperature, suction filtration, by filter cake nothing
Water-ethanol, deionized water are washed 2-3 times successively, air drying, are mixed with remaining each raw material, are stirred, in feeding extruder,
Melting extrusion, cooling, obtains final product the antibacterial type polyurethane waterproof material.
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Application publication date: 20170609 |